Determination of pharmaceuticals, steroid hormones, and endocrine-disrupting personal care products in sewage sludge by ultra-high-performance liquid chromatography–tandem mass spectrometry

AbstractA sensitive method has been developed and validated for the determination of diverse groups of pharmaceuticals, steroid hormones, and hormone-like personal care products in sewage sludge. Samples were extracted by ultrasonic-assisted extraction followed by solid-phase extraction cleanup. For determination of estrogens and hormone-like phenolic compounds, sample extracts were further derivatized with dansyl chloride and purified with silica gel column chromatography to improve the analytical sensitivity. The chemicals were determined by ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) in multiple-reaction monitoring mode. Recoveries ranged mostly from 63% to 119% with relative standard deviations within 15%. Method quantification limits were 0.1–3 ng g−1 dry weight (dw) for sewage sludge. The method was applied to a preliminary investigation of pharmaceuticals and personal care products (PPCPs) in sewage sludge and sediment in the Pearl River Delta, South China. Triclosan, triclocarban, 2-phenylphenol, bisphenol A, and parabens were ubiquitously detected at 3.6–5088.2 ng g−1 dw in sludge and 0.29–113.1 ng g−1 dw in sediment samples, respectively. Estrone, carbamazepine, metoprolol, and propranolol were also frequently quantified in the sludge and sediment samples. The dewatering process caused no significant losses of these PPCPs in sewage sludge. FigureMRM chromatograms of the analytes in a standard solution at 5 ng mL−1 (A), sewage sludge (B), river sediment (C), and estuary sediment (D) samples. ATL, atenolol; MPL, metoprolol; CBZ, carbamazepine; E1, estrone; E2,17β-estradiol, E3, estriol; EE2,17α-ethynylestradiol; MedP, medroxyprogesterone; MP, methylparaben; EP, ethylparaben; PP, propylparaben, PHP, 2-phenylphenol; TCS, triclosan; TCC, triclocarban; BPA, bisphenol A.